KR930000238B1 - Manufacturing process of composite fiber - Google Patents

Abstract

forming first component of fiber- forming polyamide resin in a way the polyamide resin forms radial portions by branching it radially in 4-8 directions from the center of cross-section; forming second component of thermoplastic polyester resin forming wedge portion alternately between first components, containing inorganic particles of SiO2 of 5 mμ - 50 mμ, the content per polyester resin 0.1-3.0 wt.%, resulting in forming multiple concave-convex shapes of 0.4-0.8 μ along the fiber-axis upon alkali wt. redn., and also copolymerized with 0.3-3.0 mol% organic acid copolymerizing cpd. of formula (I) [where R1=R2=CnH2n+1 (n = 1-10) or (CH2)mOH (m = 2-10); M= alkali metal with terephthalic acid and containing metal sulphomate group, alkali wt. reducing, and forming resin film of refractive index 1.4-1.6, e.g. polyurethane.

Description

Manufacturing method of composite fiber structure

1 to 3 is an enlarged cross-sectional view of the composite fiber of the present invention

A: Fiber-forming polyamide resin

B: fiber-forming polyester resin

The present invention is salty to basic dyes and has a number of fine irregularities of optical wavelength order in the fiber axis direction by alkali reduction treatment on the fiber surface and forms a resin film of low refractive index in comparison with general microfine fibers when dyeing. The present invention relates to a method for producing a polyamide-polyester-based composite microfiber structure that can exhibit a significant deep color effect and high color development.

In general, microfibers of less than 0.3 denier have a wide variety of uses such as artificial suede, moisture-permeable and waterproof fabrics, and clean fabrics, but there are difficulties in the process of dyeing and processing.

Microfibers are known to have a lower apparent surface concentration (chromic) than conventional fibers, which is a common problem with microfibers. As the decrease in the apparent concentration, as the fiber becomes thinner, the surface area with respect to the unit weight increases and the reflected light on the surface of the fiber increases, so that the light scatters and the colored light is weakened, so that the apparent density of the surface is lowered. However, if the apparent concentration is lowered, the use of a high concentration of salt does not give the color development equivalent to that of regular denier fibers.

On the other hand, as a method for imparting irregularities to the surface of the fiber to improve color development, the method of adding polymers of inert fine particles and crystallization agents disclosed in Japanese Patent Application Laid-Open Nos. 43-14186 and 46-26887 and Japanese Patent Publication No. 43-16665 Solvent treatment after the addition of fine particles is known, but such a method is difficult to obtain a sufficient deep color effect by forming irregularities of several to tens of times the wavelength of light on the fiber surface. In addition, the method disclosed in Japanese Patent Application Laid-Open No. 55-137241 is formed in the circumferential direction perpendicular to the fiber axis to reduce tearing and tensile strength of the fiber structure, and has a deep color effect only by surface irregularities due to the high refractive index of the polyester fiber itself. There is not enough to gain.

In order to solve these drawbacks, the present inventors are soluble in basic dyes and elute the fine particles in the alkali reduction process to form fine irregularities of 0.4 ~ 0.8μ, which are light wavelength orders, on the surface of the fiber to diffuse light diffusely and form a resin film having a low refractive index. By inventing a method for producing a highly colored polyamide-polyester-based composite microfiber structure to minimize the reflected light.

The present invention is described in detail as follows.

The present invention relates to a fiber-forming polyamide resin as a first component in a multi-segment composite fiber composed of fiber-forming polyamide and fiber-forming polyester. As shown in the figure, radially branched from the center of the cross section of the composite fiber to form a radial portion of four directions or more and eight directions or less, and the second component, the fiber-forming polyester resin, alternates with the first component between the first component. It is arranged to form a wedge, and the second component contains inorganic particles having an average diameter of 5 mμ to 50 mμ to form a large number of fine irregularities on the fiber surface during alkali reduction and at the same time, a metal sulfo having affinity with basic dyes. A thermoplastic polyester resin copolymerized with an organic acid containing an nate group was used, and after the alkali reduction of the composite fiber, a resin film having a refractive index of 1.4 to 1.6 was formed. Characterized in that the rock.

Inorganic particles used in the present invention are silicon oxide dispersed in water, the average particle diameter of less than 5mμ is not enough effect of the unevenness after reducing the alkali, and the price of the dispersion itself is expensive, it is difficult to put to practical use, the 50mμ or more is more than light wavelength Too large unevenness results in insufficient light scattering effect, and the strength deterioration of the fiber is remarkable.

The content of the non-particles may vary depending on the shape and density of the desired irregularities after the weight loss process, but 0.1 to 3% by weight of the polyester resin is suitable to prevent splitting and trimming during spinning. If the content is less than 0.1% by weight, the formation of unevenness is insufficient, and it does not help color development after dyeing. If the content is more than 3% by weight, the segment is separated during the weaving process, so that not only the bleeding occurs but also severe cutting occurs. Trimming occurs during the shaving process, causing unstable operation and defects.

In addition, after the reduction of alkali, the strength decreases remarkably, and thus does not function as a fiber product.

The present invention is a composite spinning of a fiber-forming polyester resin and a fiber-forming polyamide resin copolymerized with an organic acid containing a metal sulfonate group while containing the inorganic particles described above, the total fineness of 50 ~ 150 denier, single yarn fineness 1-3 denier After weaving or weaving, dividing and minimizing by chemical or physical method, fine inorganic irregularities are formed by extracting inorganic particles by alkali reduction process, and then applying a low refractive index resin film on the surface of the fiber for basic dyeing. To improve the color and color development.

The chemical method of dividing is dividing or dividing the solvent selectively acting on the two-component polymer forming the fiber, the solvent used is benzyl alcohol, phenyl ethyl alcohol (phenyl ethyl alcohol, phenol, ortho chlorophenol, m-cresol, para-cresol, alpha methyl alcohol, ortho phenyl phenol (O-phenyl phenol) is known, but benzyl alcohol is known to be suitable in consideration of stability, workability, price, etc. As a physical method, dividing by entangled brushing and buffing is a typical method. As a method used in the manufacture of suede. In some cases, chemical and physical methods may be combined.

In general, the loss of alkali of polyester fiber is increased by hydrolysis of ester groups in the polyester polymer chain to form terephthalic acid and ethylene glycol, and neutralization of terephthalic acid to disodium terephthalate. A decrease occurs, and hydrolysis is known to occur slowly from the fiber surface due to the compactness of the polyester fiber structure because the rate of alkali decomposition is faster than the penetration rate of alkali into the fiber. Inorganic particles are distributed on the surface of the polyester fiber, and the structure around the inorganic particles is loosened due to micro voids and the like, so that the hydrolysis effect is increased. In the end, the inorganic particles are eluted out of the fiber and fine on the fiber surface. Unevenness is formed. Fine unevenness scatters the light when the light is incident on the fiber, thereby reducing the reflected light on the surface of the fiber, that is, the white light, which in turn increases the colored light of the dyeing, resulting in high color development.

Polyester fiber is a high-temperature high-pressure dyeing by the disperse dye is common, which is difficult to show a vivid color due to the low color development of the disperse dye itself, there is a drawback that takes a lot of energy. In order to improve this, there is known a method of preparing modified polyester fibers salted with basic dyes capable of vivid dyeing by copolymerizing an organic acid containing a metal sulfonate group.

In the present invention, as an organic acid containing a metal sulfonate group used as a polymerization modifier for basic salting, a compound represented by the following formula (I) was copolymerized with 0.3 to 3.0 mole% of terephthalic acid.

Wherein R _1, R ₂ is _{C n H 2n + 1 (n} = an integer of 1 to 10), or (CH ₂₎ m OH (integer m = 2 ~ 10), M is an alkali metal.

If the amount is less than 0.3 mol%, there is a lack of seats capable of dyeing basic dyes, and thus color development cannot be expected. The physical property of) is remarkable and the alkali loss resistance is insufficient, making it difficult to control the alkali reduction process.

Polyester fibers have the highest refractive index among the fibers, which is one factor that hinders the color development of the polyester fibers. As another method of improving the deep color of a polyester fiber, when the low refractive index resin of refractive index 1.4-1.6 is apply | coated to a fiber surface, it is known that the surface reflectance of light falls and color development and color depth improve. Low refractive index resins include fluorine-based compounds, mixtures of silicon oxide and hydrophilic vinyl monomers, mixtures of silicon oxide and water-soluble polyamide resins, polyurethane resins, mixtures of polyurethane and silicone compounds, and the like. Is proposed.

Inorganic particles used for the purpose of forming the irregularities in the present invention is a colloidal silica having a silicon oxide content of 10 to 50% by weight of finely dispersed silicon oxide (SiO ₂ ) having a uniform particle diameter of 5 μm to 50 μm in water and a hydrogen ion concentration of 9.0 to 11.0 ( Colloidal Silica) was used and added at any stage during the polymerization of the polyester resin.

The alkali weight loss was appropriately divided by chemical or physical method and then carried out by a known method to reduce 5 to 15% by weight of the fiber. Considering the polyamide component, the weight was reduced by 7 to 20% based on the polyester component.

The single yarn fineness of the polyester component after the dividing treatment is less than 0.3 denier, and the surface area is larger than that of the regular denier fiber, which is to be performed under mild conditions or to reduce the reduction time. In addition, when the dividing process is performed with benzyl alcohol, micro voids in the fiber formed by the benzyl alcohol treatment increase the surface area, thereby increasing the number of collisions of the OH group and facilitating the penetration of the hydroxyl group into the fiber. As the decomposition effect is increased, it is necessary to make the processing conditions more mild.

As the low refractive index resin used in the present invention, a thermally-reactive polyurethane was used in consideration of dry cleaning durability and touch, and this polyurethane was a self-emulsifying urethane prepolymer in which isocyanate was sealed with bisulfite. Urethane obtained by reacting a block or random copolymer polyether diol of propylene oxide and ethylene oxide with hexamethylene diisocyanate or xylene diisocyanate The thing which blocked the terminal isocyanate group of prepolymer with bisulfite is mentioned, for example.

The amount of the urethane is preferably to be attached to the resin solid content of 0.1 to 5.0% by weight based on the weight of the fiber.

Hereinafter, the present invention will be described in detail with reference to Examples.

Example 1

The relative viscosity is 2.6 in nylon 20 at 20 ° C. and 96% sulfuric acid as the first component, and 5-sodium sulfo di (2-hydroxy ethyl) isophthalate is used. 1.5 mol% copolymerized with terephthalic acid, containing 1 wt% of silicon oxide having an average particle diameter of 15 mμ, and having an intrinsic viscosity of 0.64 in polyethylene terephthalate (O-Chlorophenol) as a second component 1: Melt-spun at a volume ratio of 3 and wound at a speed of 1,500 m / min to obtain an undrawn yarn having a cross-sectional shape as shown in FIG. This was stretched three times at 130 ° C. and heat-fixed with a hot plate at 150 ° C. to obtain 75 denier 36 filament multisegment composite fibers.

Weaving is carried out in a plain manner using regular polyethylene terephthalate fibers of 75 denier 36 filaments as a warp yarn and a composite weft yarn of the former. After dividing in a benzyl alcohol emulsion dispersion so as to have a split ratio of 90% or more, the reduction ratio is 10. It was boiled with aqueous sodium hydroxide solution so as to be%. The alkaline treated fabric was padded in a 10% aqueous solution (1.5% solids) of a water-soluble urethane free polymer "ELASTRONC-52" (Cheil Industries, Ltd.), and made into a mangle so that the pick-up was 70%. After squeezing and drying at 80 ° C. for 2 minutes, heat treatment was performed at 160 ° C. for 1 minute.

The treated fabric was dyed for 1 hour at 120 ° C using basic dye Kayacryl blue BM-ED (3% owf) at a concentration of 3% owf to reduce the uneven size, color development and strength of the dyed fabric. The results are shown in Table 1 below.

Comparative Example 1

The same process as in Example 1 was carried out except that the silicon oxide was not contained in Example 1. The results are shown in Table 1.

Comparative Example 2

In Example 1, the same method as in Example 1 was carried out except that the silicon oxide content was 0.05% by weight. The results are shown in Table 1.

Comparative Example 3

The same process as in Example 1 was carried out except that the silicon oxide content was contained in 5.0 wt% in Example 1. The results are shown in Table 1.

Comparative Example 4

The same procedure as in Example 1 was carried out except that the water-soluble urethane prepolymer treatment was not performed in Example 1. The results are shown in Table 1.

TABLE 1

Assessment Methods

1. Uneven size

By scanning electron microscopy The negative axial length was measured.

2. Color development

Compared with the standard fabric, the degree of improvement in color development was determined. The standard fabric was made to contain no silicon oxide in the second component in Example 1, no alkali loss processing after the split treatment, and no water-soluble urethane prepolymer treatment. Was prepared in the same manner as in Example 1. The obtained dyeing cloth was observed under natural light, and 10 judges were selected according to the following judgment criteria, and the sensory test was carried out, and these values were averaged and taken as judgment values.

Class 1: Color development is not improved compared to standard cloth.

2nd class: Color development is slightly improved compared to standard cloth.

Class 3: Color development is significantly improved compared to standard pouch.

3. Strength reduction rate

The percentage of tear strength and tensile strength of the weft of the standard fabric was expressed as a percentage, and the calculation was performed as follows.

Here, the tear strength was evaluated by KS K 0535 (Pendulum Method) and tensile strength KS K 0520 (Rabble Strip Method).

4. Radioactive

The evaluation was performed by considering the operability such as splitting, mooring and trimming.

Claims (4)

In the multi-segmented composite fiber made of fiber-forming polyamide and fiber-forming polyester, the first component, the fiber-forming polyamide-based resin is branched radially from the center of the cross section of the fiber in four directions. The above-mentioned radial direction of 8 directions or less is formed, and the fiber-forming polyester resin which is a 2nd component is arrange | positioned alternately with a 1st component between a 1st component, and forms a wedge-shaped part. When the weight loss, a thermoplastic polyester resin in which a plurality of unevennesses in the fiber axis direction are formed in the fiber axis direction and the organic acid containing a metal sulfonate group having affinity with basic dyes is used is used. A method for producing a composite fiber structure exhibiting high color development after dyeing by forming a resin film having a low refractive index after alkali reduction of the composite fiber. The method for producing a composite fiber structure according to claim 1, wherein the inorganic fine particles are 5 m to 50 m m of silicon oxide (SiO ₂ ) and the content is 0.1 to 3.0 wt% based on the polyester resin. The method of claim 1, wherein the organic acid containing a metal sulfonate group having affinity with a basic dye is copolymerized with 0.3 to 3.0 mol% of terephthalic acid with a compound represented by the following formula (I): Method for producing a composite fiber structure. R ₁ and R ₂ are C _n H _{2n + 1} (an integer of n = 1 to 10) or (CH ₂ ) mOH (an integer of m = 2 to 10) M is an alkali metal. The method for producing a composite fiber structure according to claim 1, wherein the low refractive index resin film is a polyurethane having a refractive index of 1.4 to 1.6.